Compressibility of β-As4S4: an in situ high-pressure single-crystal X-ray study

GO Lepore, TB Ballaran, F Nestola… - Mineralogical …, 2012 - pubs.geoscienceworld.org
GO Lepore, TB Ballaran, F Nestola, L Bindi, D Pasqual, P Bonazzi
Mineralogical Magazine, 2012pubs.geoscienceworld.org
Ambient temperature X-ray diffraction data were collected at different pressures from two
crystals of β-As 4 S 4, which were made by heating realgar under vacuum at 295 C for 24 h.
These data were used to calculate the unit-cell parameters at pressures up to 6.86 GPa.
Above 2.86 GPa, it was only possible to make an approximate measurement of the unit-cell
parameters. As expected for a crystal structure that contains molecular units held together by
weak van der Waals interactions, β-As 4 S 4 has an exceptionally high compressibility. The …
Abstract
Ambient temperature X-ray diffraction data were collected at different pressures from two crystals of β-As 4 S 4, which were made by heating realgar under vacuum at 295 C for 24 h. These data were used to calculate the unit-cell parameters at pressures up to 6.86 GPa. Above 2.86 GPa, it was only possible to make an approximate measurement of the unit-cell parameters. As expected for a crystal structure that contains molecular units held together by weak van der Waals interactions, β-As 4 S 4 has an exceptionally high compressibility. The compressibility data were fitted to a third-order Birch–Murnaghan equation of state with a resulting volume V 0= 808.2 (2) Å 3, bulk modulus K 0= 10.9 (2) GPa and K′= 8.9 (3). These values are extremely close to those reported for the low-temperature polymorph of As 4 S 4, realgar, which contains the same As 4 S 4 cage-molecule. Structural analysis showed that the unit-cell contraction is due mainly to the reduction in intermolecular distances, which causes a substantial reduction in the unit-cell volume (~ 21% at 6.86 GPa). The cage-like As 4 S 4 molecules are only slightly affected. No phase transitions occur in the pressure range investigated.
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